EP0662108B1 - Procede pour ameliorer la compatibilite de silices precipitees avec des aromes - Google Patents

Procede pour ameliorer la compatibilite de silices precipitees avec des aromes Download PDF

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Publication number
EP0662108B1
EP0662108B1 EP93920813A EP93920813A EP0662108B1 EP 0662108 B1 EP0662108 B1 EP 0662108B1 EP 93920813 A EP93920813 A EP 93920813A EP 93920813 A EP93920813 A EP 93920813A EP 0662108 B1 EP0662108 B1 EP 0662108B1
Authority
EP
European Patent Office
Prior art keywords
silica
flavour
silicas
precipitated
treated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP93920813A
Other languages
German (de)
English (en)
Other versions
EP0662108A1 (fr
Inventor
Nand Sanmukhdas D-5 Mira Mansion Bijlani
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GB929220151A external-priority patent/GB9220151D0/en
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0662108A1 publication Critical patent/EP0662108A1/fr
Application granted granted Critical
Publication of EP0662108B1 publication Critical patent/EP0662108B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size

Definitions

  • the present invention relates to an improvement in the flavour compatibility of precipitated silicas, used in dental care products such as dentifrices.
  • silicas are frequently used, for several purposes. They are mainly synthetic silicas, of which the three main types are pyrogenic silicas, precipitated silicas, and silica gels (aerogels, xerogels and hydrogels). These silicas are used as abrasive agents or as thickening agents in dentifrices. For imparting abrasive and thickening properties to dentifrices, particularly to gel-type dentifrices, precipitated silicas are the most frequently used. The present invention is particularly concerned with such precipitated silicas.
  • Precipitated silicas are commonly prepared by precipitating them from dilute sodium silicate solutions by the addition of mineral acid and sometimes salt, followed by washing with water and drying. They mainly differ from the pyrogenic silicas and silica gels in that they have a much smaller surface area (e.g. 150-450 m 2 /g) and a much larger pore volume (e.g. 0.4-1.0 ml/g) than the pyrogenic silicas or the silica gels (e.g. 600-800 m 2 /g and 0.2-0.4 ml/g). Also the average pore size is different (more than 2 nm compared with 1-1.2 nm)
  • Dental care products such as dentifrices almost invariably also contains flavours added thereto, but we have found that the impact of such flavours is much less pronounced in dentifrices that contain precipitated silicas than in dentifrices that contain one of the other types of synthetic silicas, e.g. abrasive silicas of the silica gel type.
  • flavour impact of flavours present in a dentifrice that also contains a precipitated silica.
  • this object can be achieved to a significant extent by improving the compatibility of such precipitated silicas with flavours.
  • This improved compatibility is achieved by treating the precipitated silica with an alkaline material.
  • the present invention relates to a process for improving the compatibility of precipitated silicas with flavours, wherein said silicas are treated with an alkaline material.
  • a further object of the invention is to improve the foaming power and creaminess of the foam of a dentifrice that comprises a detergent-active material by inclusion therein of an alkali-treated precipitated silica, which produces a synergistic interaction with the detergent-active material.
  • the treatment of the precipitated silicas with an alkaline material according to the present invention should take place after the precipitated silica has been dried.
  • the dried precipitated silica can for instance be slurried with water and a suitable amount of an alkaline material can then be added to the slurry, whereupon the treated silica can be filtered off and dried.
  • spray-drying or flash drying is the preferred method to achieve a product which matches closely the original precipitated silica in terms of particle size and slurry viscosity.
  • the dried precipitated silica may also be added to a dentifrice formulation during the manufacture thereof, said formulation containing a suitable alkaline material, prior to the incorporation of a flavour to such dentifrice formulation.
  • This can be done by in-situ treatment of the silica with the alkaline material in the presence of humectants during the dentifrice processing.
  • Preferred, however, is the separate treatment of the dried silica with the alkaline material.
  • Suitable alkaline materials are sodium hydroxide, potassium hydroxide, sodium or potassium carbonate, sodium or potassium bicarbonate, sodium fluoride, tetrasodiumpyrophosphate, sodium trimetaphosphate, ammonia, organic amines and so on.
  • a 10% aqueous slurry of the silica has a pH of between 7.0 and 10.0, preferably 7.0 and 8.5, preferably between 7.5 and 8.5 and particularly preferably between 8.0 and 8.5.
  • the alkali-treated precipitated silica of the invention is particularly useful in flavour-containing dental care products such as dentifrices. They are usually included therein in an amount of from 1-25%, commonly in an amount of 5-20% by weight. They are suitable for inclusion in both gel-type dentifrices as in non-gel type dentifrices. Both types of dentifrices may contain the usual additional ingredients in conventional amounts. Thus, as dentifrice it will usually comprise an abrasive cleaning agent in an amount of from 3-75% by weight.
  • Suitable abrasive cleaning agents are milled or unmilled particulate aluminas; silica xerogels, hydrogels and aerogels; precipitated silica; calciumpyrophosphate; insoluble sodium metaphosphate; calcium carbonate; dicalcium orthophosphate; particulate hydroxyapatite and so on.
  • the dentifrice may contain a liquid phase comprising water and a humectant in an amount of 10-99% by weight.
  • Typical humectants are glycerol, sorbitol, polyethyleneglycol, polypropylene glycol, propylene glycol, hydrogenated partially hydrolyzed polysaccharides and so on.
  • Binders or thickening agents such as sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, xanthan gums, Irish moss, gum tragacanth, finely-divided hectorites may also be included in the dentifrice in an amount of 0.5 -10% by weight.
  • Another conventional ingredient in a dentifrice is an organic surfactant such as a soap, an anionic, nonionic, cationic, ampholytic and/or a zwitterionic synthetic detergent surfactant in an amount of 0.2-5% by weight.
  • compositions of the invention may be included in the compositions of the invention, e.g. sweetening agents such as sodium saccharinate, whitening agents such as titanium dioxide or zinc oxide, preservatives, vitamins such as vitamin C and E, anti-plaque agents such as zinc salts like zinc citrate, copper salts, stannous salts like stannouspyrophosphate, sanguinarine, allantoin, p-aminobenzoic acid derivates, hexetidine, chlorhexidine, 3-(4-propylheptyl)- 4-(2-hydroxyethyl)- morpholine, antibacterial agents such as Triclosan (2',4,4'-trichloro-2-hydroxy-diphenyl ether), anti-calculus agents such as di- and/or tetra-alkalimetalpyrophosphates, pH adjusting agents, colouring agents, anti-caries agents such as casein, casein digests, sodium trimetaphosphate, sodium fluoride and monosodiumfluoro
  • Flavours to be used in the present invention can be any of the commonly used, well-known flavours for dentifrices such as peppermint oil, spearmint oil, menthol, carvone and so on. Flavours are usually used in an amount of 0.01 - 2%.
  • Equilibrium head space gas chromatography was used to determine the vapor phase composition of flavour in equilibrium with the silica.
  • the flavour-adsorbed silica in equilibrium with flavour vapours was taken into a head space vial of 50 ml capacity.
  • the sealed vial was equilibrated at 50°C for 20 minutes.
  • An aliquot of the head space was injected into the GC column.
  • the chromatogram was processed by a computing integrator. The area given by the pure flavour was taken as standard and the results were normalised.
  • QDA Qualitative descriptive analysis
  • This is carried out by a panel consisting of 15-16 people trained to evaluate toothpaste performance.
  • the product attributes assessed in this method are foam amount, foam creaminess, flavour impact, pungency, mouth freshness, cooling after brushing, paste spreadability, grittiness, etc.
  • the protocol for brusing involves taking half a brush length of the sample on a pre-wetted brush and brushing for 60 seconds. Panelists are asked to assess each of the attributes and rate them on a ten point scale. The mean rating for each attribute is calculated and plotted on a QDA chart, whereby comparative evaluation of overall performance of toothpaste samples can be done.
  • the example shows that the toothpaste composition containing modified thickening silica has a synergistic effect with the flavour and detergent giving rise to better foam and flavour impacts.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Inorganic Chemistry (AREA)
  • Epidemiology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)
  • Silicon Compounds (AREA)

Abstract

La compatibilité de silices précipitées avec des arômes peut être notablement améliorée par traitement des silices avec un matériau alcalin. Les silices précipitées ainsi traitées présentent une compatibilité améliorée avec les arômes, ce qui est particulièrement avantageux dans les dentifrices.

Claims (5)

  1. Procédé pour améliorer la compatibilité des silices précipitées avec les arômes, comprenant le traitement des silices précipitées séchées avec une matière basique.
  2. Procédé selon la revendication 1, dans lequel la matière basique est l'hydroxyde de sodium.
  3. Procédé selon la revendication 1, dans lequel les silices précipitées séchées sont traitées avec la matière basique dans une suspension aqueuse, qui est ultérieurement éliminée par filtration, après quoi les silices traitées sont séchées par pulvérisation.
  4. Procédé pour la préparation d'une composition dentifrice aromatisée consistant à mélanger les ingrédients de la composition de dentifrice, dans lequel on mélange les ingrédients avec un arôme et une silice précipitée séchée que l'on a traitée avec une matière basique selon l'une quelconque des revendications 1 à 3.
  5. Procédé selon la revendication 4, dans lequel on prépare une composition de dentifrice contenant une silice abrasive du type gel et une silice épaississante précipitée séchée traitée avec une base.
EP93920813A 1992-09-24 1993-09-22 Procede pour ameliorer la compatibilite de silices precipitees avec des aromes Expired - Lifetime EP0662108B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB929220151A GB9220151D0 (fr) 1992-08-12 1992-09-24
GB9220151 1992-09-24
PCT/EP1993/002591 WO1994006868A1 (fr) 1992-09-24 1993-09-22 Procede pour ameliorer la compatibilite de silices precipitees avec des aromes

Publications (2)

Publication Number Publication Date
EP0662108A1 EP0662108A1 (fr) 1995-07-12
EP0662108B1 true EP0662108B1 (fr) 1997-02-26

Family

ID=10722412

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93920813A Expired - Lifetime EP0662108B1 (fr) 1992-09-24 1993-09-22 Procede pour ameliorer la compatibilite de silices precipitees avec des aromes

Country Status (7)

Country Link
EP (1) EP0662108B1 (fr)
CN (1) CN1091629A (fr)
AU (1) AU670961B2 (fr)
BR (1) BR9307083A (fr)
DE (1) DE69308312D1 (fr)
WO (1) WO1994006868A1 (fr)
ZA (1) ZA937037B (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2751635B1 (fr) * 1996-07-23 1998-10-02 Rhone Poulenc Chimie Silice compatible avec les aromes, son procede de preparation et compositions dentifrices la contenant
EP2349489B1 (fr) 2008-11-25 2015-11-11 The Procter and Gamble Company Compositions de soin buccal à faible ph contenant de la silice fondue et une source de fluorure
US8551457B2 (en) 2008-11-25 2013-10-08 The Procter & Gamble Company Oral care compositions comprising spherical fused silica
US20110293541A1 (en) 2010-05-25 2011-12-01 John Christian Haught Oral Care Compositions And Methods Of Making Oral Care Compositions Comprising Silica From Plant Materials
CN104768520B (zh) 2012-11-05 2017-06-13 宝洁公司 热处理的沉淀二氧化硅
BR112016013531A8 (pt) 2013-12-20 2020-05-19 Colgate Palmolive Co composição de cuidado oral
AU2014369061B2 (en) 2013-12-20 2017-03-02 Colgate-Palmolive Company Tooth whitening oral care product with core shell silica particles

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4421527A (en) * 1977-12-20 1983-12-20 J. M. Huber Corporation High fluoride compatibility dentifrice abrasives and compositions

Also Published As

Publication number Publication date
DE69308312D1 (de) 1997-04-03
ZA937037B (en) 1995-03-23
BR9307083A (pt) 1999-03-30
CN1091629A (zh) 1994-09-07
AU4819193A (en) 1994-04-12
EP0662108A1 (fr) 1995-07-12
AU670961B2 (en) 1996-08-08
WO1994006868A1 (fr) 1994-03-31

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